Patent application title: Stabilized vitamin solutions; use thereof; process for their production; and formulations comprising the same

Abstract:

This invention relates to improved composition and method for producing
individual dosages of nutritional supplements containing a large dose of
stable ascorbic acid, vitamins and herbal extracts having extended shelf
life without substantial degradation for mammals. The process involves
heating a mixture of ascorbic acid and a humectant to elevated
temperature with agitation to stabilize ascorbic acid at selected water
activity.

Claims:

1. A composition of a stabilized ascorbic acid solution comprising:a)
ascorbic acid and/or one of its derivatives; andb) glycerin

2. The composition of claim 1, wherein the ascorbic acid and glycerin are
heated to about 130 F or above to dissolve ascorbic acid.

3. The composition of claim 1, wherein the ascorbic acid concentration is
about 25% (w/w) or less in solution,

4. The composition of claim 1, wherein the glycerin concentration is about
10 to 95% (w/w) in solution.

11. The composition of claim 5, wherein the added optional ingredients is
selected from the group consisting of sweeteners, flavors and colors or
combinations thereof.

12. A process for obtaining a stabilized ascorbic acid solution of a
desired stability, which comprises:a) mixing ascorbic acid and/or one of
its derivatives and a humectant;b) adding sufficient humectant to lower
water activity of solution to about 0.60 or below;c) heating to about 120
F or above to dissolve ascorbic acid

13. The process of claim 12, wherein the humectant is selected from a
group consisting of glycerin, reducing sugars, polyols, maltitol,
sorbitol, xylitol, mannitol, isomalt, lactitol, and erythritol or
mixtures or derivatives thereof.

14. The process of claim 12, wherein the process further comprises adding
between about 5% to 45% water.

15. A kit comprising a preformed package, the kit comprising:dissolved
ascorbic acid and/or one of its derivatives and humectant.

16. The kit of claim 15, wherein the preformed package is hermetically
sealed.

17. The kit of claim 15, wherein the composition is a single serve
concentrated nutritional supplement to be diluted in water.

18. The kit of claim 15, wherein the glycerin is present at 30 to 95%.

19. The kit of claim 15, wherein the water activity is about 0.60 below.

20. The kit of claim 15, wherein the humectant is selected from a group
consisting of glycerin, reducing sugars, polyols, maltitol, sorbitol,
xylitol, mannitol, isomalt, lactitol, and erythritol or mixtures or
derivatives thereof.

Description:

FIELD OF INVENTION

[0001]The present invention relates to composition of stabilized ascorbic
acid and nutritional supplement solutions, use thereof, process for their
production, and formulations comprising the same. This invention further
relates to a process for manufacturing concentrated stabilized ascorbic
acid and vitamin solutions in single dose unit with long shelf-life.

BACKGROUND

[0002]Vitamin C (ascorbic acid) is a vital nutrient for humans and has
many important functions in-the body. Vitamin C is essential for collagen
synthesis and helps maintain the integrity of substances of mesenchymal
origin, such as connective tissue, osteoid tissue, and dentin. An
essential function of ascorbic acid is to act as a cofactor for the
hydroxylation of proline and lysine residues in collagen, a major protein
component of the body that is important in maintaining healthy skin
elasticity and texture. Ascorbic acid is further essential for wound
healing and facilitates recovery from burns. Being a strong reducing
agent, ascorbic acid is reversibly oxidized and reduced in the body,
functioning as a redox system in the cell and being useful in the
treatment of cancer. It is involved in the metabolism of phenylalanine
and tyrosine. Vitamin C facilitates the absorption of iron and protects
folic acid reductase, which converts folic acid to folinic acid, and may
help release free folic acid from its conjugates in food.

[0003]Vitamin C is a powerful antioxidant, protecting against oxidative
damage to DNA, membrane lipids and proteins. As mentioned above, it is
involved in the synthesis of numerous substances such as collagen, and
also of certain anabolic steroid hormones, and transmitters of the
nervous system, lipids and proteins. It seems to be required for proper
immune function and its use has been recommended to prevent or treat
colds. Although this has not been demonstrated by experimental studies,
it seems that Vitamin C does shorten or reduce the severity of a cold.
Vitamin C is also a water-soluble cellular antioxidant that reacts with
free radicals in the water compartment of cells and in intercellular
fluids and can "recycle" vitamin E by chemically regenerating it after it
has been spent in terminating a free radical reaction.

[0004]Vitamin C (L-ascorbic acid) is a moderately strong reducing agent,
which makes it unstable in aqueous solutions, especially at high pHs. It
is particularly subject to oxidative degradation.

[0005]L-ascorbic acid is chemically defined as an alpha-ketolactone with
the following chemical structure: The number 2 and 3 carbons are
double-bonded and contain acid-ionizable hydrogen in water (pK=4.2).
Ascorbic acid is moderately strong reducing agent. Unfortunately, these
properties lead to instability in the ascorbic acid structure which is
burdensome to formulators attempting to prepare ascorbic acid solutions
such as aqueous solutions. In particular, at higher pH's, the ascorbic
acid increasingly becomes the unstable ascorbate anion (the conjugate
base of ascorbic acid), which is susceptible to degradation.

[0006]L-ascorbic acid limit of solubility in water appears to be about 330
mg/ml in water. L-ascorbic acid is therefore relatively soluble in water.
It is much less soluble in glycols such as propylene glycol (50 mg/ml)
and in alcohols such as ethanol (10 mg/ml in absolute ethanol) and
insoluble in glycerin as stated in the prior art. Although water is the
best solvent to provide an ascorbic acid solution, it is one of the worst
to protect ascorbic acid against oxidative damages. A proportion of water
needs to be replaced with another solvent that provides more stability.
The dilemma with ascorbic acid formulations has always been to find a
balance between solubilization and stability.

[0007]The instability of L-ascorbic acid may be caused by a number of
factors including stereo chemical strain. For example, when the 2-hydroxy
group ionizes, it places two negative charges in close proximity which
favors ring disruption. Furthermore, oxidative degeneration likely
promotes instability due to the ascorbate anion's propensity to act as a
reductant, thus the molecule is prone to breaking down to form species
such as L-threonic acid and oxalic acid. Such breakdowns can be catalyzed
by the presence of a transition metal. Degradation may also occur due to
tap water mixing.

[0008]Various attempts have been made to produce stable solutions of
L-ascorbic acid and its salts, but have been met with poor success. Most
approaches to formulate and use ascorbic acid were related to dermatology
to produce topical treatments for skin not for direct ingestion.

[0009]U.S. Pat. No. 2,187,467 discloses aqueous solutions of ascorbic acid
stabilized by the addition of salts of alkaline earth metals, ammonium,
and soluble salt of a sulfite acid. However, this patent states that the
stabilization was not achieved with the acid itself.

[0010]U.S. Pat. No. 5,140,043 discloses an ascorbic acid formulation that
has a pH below 3.5, preferably below 2.5. A low pH insures that a high
proportion of ascorbic acid remains in the protonated, uncharged form.
The protonated form is more stable and more easily permeant through skin
and mucosae membranes than the non-protonated counterpart. Metals also
negatively influence the preponderance of the protonated form of ascorbic
acid in a solution. A chelator may therefore be added in ascorbic acid
solutions to stabilize the vitamin. The carrier in which the ascorbic
acid is dissolved comprises an alkylene glycol, namely propylene glycol.
The carrier further comprises hydroxyalkylcellulose, the polyhydroxyl
function of which apparently participates in the typical reactions of
alcohols. The proportion of water remains very high (more than 50% by
weight), which may lead to a relatively rapid degradation at room
temperature.

[0011]U.S. Pat. No. 4,983,382 discloses the use of polyhydric liquids to
solubilize and stabilize ascorbic acid. A mixture of ethanol 55-65% and
propylene glycol 20-25% is especially preferred for its excellent
cosmetic properties. Water may be present in concentrations up to 12%
without adversely affecting the stability of ascorbic acid solubilized in
a mixture of alcohol and propylene glycol. The organic solvents, all
combined, represent up to 90% by weight of a composition. The low water
contents recommended does not appear to permit solubilization of more
than 10% of ascorbic acid.

[0012]U.S. Pat. No. 6,124,348 proposes to combine ascorbic acid, a
volatile organic solvent such as isodecane and a gelling base. The
solvent does not react with or solubilize the vitamin. Such a suspension
is applied to the skin. The skin moisture penetrates the suspension and
solubilizes the ascorbic acid which then can permeate the skin layer. The
solubility of ascorbic acid in the formulation is not dealt with in this
patent.

[0013]Another type of dispersion of ascorbic acid is disclosed in U.S.
Pat. No. 6,103,267. Again, this patent does not describe a solution of
ascorbic acid.

[0014]Another approach to stabilize ascorbic acid solution has been to
decrease water activity in the same. U.S. Pat. No. 5,736,567 discloses
compositions wherein water activity is decreased below 0.85. The lowest
water activity achieved with the descriptive examples has been 0.63. At
this value, the water content is 21%, the ascorbic acid concentration is
3%, the polypropylene glycol content is 39.4% and polyethylene glycol
content is 13% (all percentages given by weight of formulation). The
aqueous phase is combined with an oil phase to provide a composition that
has a "structure". This particular formulation has been tested for its
stability. After two months at 20 degree C., 0.7% of ascorbic acid has
degraded which is fairly good compared to the same solution prepared with
28% water (3.5% degradation) and a composition also comprising 28% water
but without the glycols (6.2% degradation). The concentration of ascorbic
acid that may be present in these formulations is not higher than 10%.

[0015]U.S. Pat. No. 6,087,393 discloses a composition comprising ascorbic
acid in a mixed glycerol carrier. The glycerol carrier comprises
propylene glycol and butylene glycol, as well as a stabilizer which may
be diethylene glycol monoethylether. The preferred proportions of
propylene glycol, butylene glycol and diethylene glycol monoethylether
are 25-80%, 5-30% and 5-10%, respectively. Ascorbic acid may be present
in concentrations comprised between 2% and 15%. In these solutions, the
major glycol component is clearly propylene glycol while butylene glycol
is added as a solubilizing aid and diethylene glycol monoethylether is
added in minor proportion as a stabilizer. The stability of these
solutions is not excellent because, at best, the samples admittedly start
to develop a yellowish color after one month at room temperature.

[0016]Another approach to formulate and use ascorbic acid in dermatology
has been not to deal with its stability. U.S. Pat. No. 5,953,584 proposes
to provide separate compartments that are extemporaneously mixed together
prior to use. One compartment comprises vitamin C, the other one
comprises an aqueous phase. Once reconstituted by admixing the contents
of both compartments, ascorbic acid is provided in a solution that is
more alkaline than usual solutions of ascorbic acid. The limit of
solubility of the vitamin achieved with such a solution is close to 50%.
Further, once reconstituted, the ascorbic acid formulation comprises
about half-and-half polyethylene glycol and water.

[0017]Because most attempts to date have been made to produce stable
solutions of L-ascorbic acid and its salts were related to dermatology to
produce topical treatments for skin, no special attention had been given
to organoleptic properties of the resulting preparation for direct
consumption or the acceptability or toxicity of solvents utilized.

[0018]Propylene Glycol has a negative connotation in the food and beverage
industries because of its bitter taste, and frequently used as a solvent
for flavor ingredients. Consumers as well limit the amount of propylene
glycol consumed because it works as a laxative.

[0019]A humectant is a hygroscopic substance. It is often a molecule with
several hydrophilic groups, most often hydroxyl groups, but amines and
carboxyl groups, sometimes estrified, can be encountered as well; the
affinity to form hydrogen bonds with molecules of water is crucial here.
Since hygroscopic substances absorb water from the air, they are
frequently used in desiccation.

[0020]When used as a food additive, the humectant has the effect of
keeping the foodstuff moist. Humectants reduce the water activity of
liquid. Water activity or aw is a measurement of the energy status
of the water in a system. It is defined as the vapor pressure of water
divided by that of pure water at the same temperature; therefore, pure
distilled water has a water activity of exactly one.

[0021]There are several factors that control water activity in a system.
Colligative effects of dissolved species (e.g. salt or sugar) interact
with water through dipole-dipole, ionic, and hydrogen bonds. Capillary
effect where the vapor pressure of water above a curved liquid meniscus
is less than that of pure water because of changes in the hydrogen
bonding between water molecules. Surface interactions in which water
interacts directly with chemical groups on undissolved ingredients (e.g.
starches and proteins) through dipole-dipole forces, ionic bonds (H3O+ or
OH--), van der Waals forces (hydrophobic bonds), and hydrogen bonds. It
is a combination of these three factors in a food product that reduces
the energy of the water and thus reduces the relative humidity as
compared to pure water. Water activity is temperature dependent.
Temperature changes water activity due to changes in water binding,
dissociation of water, solubility of solutes in water, or the state of
the matrix. Although solubility of solutes can be a controlling factor,
control is usually from the state of the matrix.

[0022]Oral dosage forms of nutritional supplements remain a significant
problem for a significant segment of the population. Many individuals are
unable or unwilling to swallow a solid dosage form. This problem occurs
primarily in children and the elderly; however, problems with swallowing
are not limited to those segments of the population. Certain conditions
or disease states manifest themselves by swallowing difficulties.
Otherwise healthy individuals can also exhibit problems with swallowing.
Such swallowing difficulties irrespective of their cause can severely
compromise patient compliance.

[0023]The neutraceutical industry has long-recognized the need for a form
of oral administration, which avoids the swallowing difficulties
associated with a traditional tablet. Syrups, elixirs, microcapsules
containing slurries, chewable tablets and other novel tablet or capsule
dosage forms have been developed, nevertheless, each has its' own
disadvantages. The disadvantages include a costly process for
preparation, the limitation of delivering only a small amount of active
ingredients and/or more costly packaging materials.

[0024]Current offering of oral nutritional supplements in the market place
for the treatment of various nutritional needs include: dry pills or
capsules (requires long time for dissolving in the stomach, has
questionable absorption rate, may require several or large pills) dry
powders (require addition to large amount of fluids making them
inconvenient to carry or consume, taste is questionable), elixirs and
syrups (bulky, hard to carry, unpleasant taste has been a deterrent to
broad acceptance by consumers), chewable tablets and other chews (taste
is questionable, smaller dosage than needed may be delivered).

[0025]Chewable systems have been developed to deliver vitamins and other
nutrients; however, they are based on low water content and low water
activity for preservations. Such formulations are too firm to chew,
excessively sticky to the teeth and require long time of chewing. Edible
nutritional supplements that are chewable have to posses acceptable taste
otherwise consumption and compliance by consumers will be affected.

[0026]An ideal liquid vitamin concentrate will have to deliver sufficient
active ingredients, exhibit long stability as well as provide a
convenient and desirable way in utilization. For instance, tablet
supplements containing 1000 mg vitamin C are large in size and hard to
swallow. Such a high dosage represents a challenge to consumers who will
have to swallow numerous large pills. A novel delivery system is needed
to deliver elevated concentrations of active ingredients in an easy to
swallow fashion with acceptable taste and flavor. That system will offer
convenience and improve compliance of utilization. There is a need to
provide a preparation that is stable over long storage under adverse
conditions. Accordingly, there is a need for an improved nutritional
supplement that can promote a healthy lifestyle and avoid drawbacks of
prior art.

SUMMARY

[0027]The present invention relates to composition and method for
producing individual dosages of stabilized ascorbic acid and other
vitamins for mammals.

[0028]The method of the present invention includes the making of a
composition for dispensing high dose of vitamins and herbs in
concentrated forms that may be reconstituted in water and ingested.

[0029]The present invention relates to composition and method for
producing individual dosages of stabilized ascorbic acid and other
vitamins characterized by high concentration for mammals.

[0030]The method of the present invention includes a process for making a
fluid composition for dispensing high dose of nutritional ingredients in
an edible format that is portable and consumable at any place.

[0031]The method of the present invention also includes methods for making
a composition for dispensing high dose of vitamin C and other vitamins
that exhibit unusual stability over prolonged period of time under
adverse conditions.

[0032]A further embodiment includes a kit comprising a pre-formed
hermetically sealed package. The kit includes a stable vitamin C and
humectants including glycerin.

[0033]Other objects, features and advantages of the present invention will
be apparent from these summary and description of preferred embodiments,
and will be readily apparent to those skilled in the art having knowledge
of gelled products/compositions and their methods of preparation. Such
objects, features, benefits and advantages will be apparent from the
above as taken in conjunction with the accompanying examples, tables,
data and all reasonable inferences to be drawn there from.

[0035]The present invention includes compositions for manufacturing
concentrated stabilized liquid ascorbic acid and other nutritional
supplements solutions with long shelf-life.

[0036]Further embodiment of the invention is a process for stabilizing
ascorbic acid for storage; the process comprising combining a further
process for stabilizing L-ascorbic acid for storage comprises combining
vitamin C and humectants including glycerin, heating the mixture to about
130 F or above, then adding water and fat soluble vitamins, herbal
extracts, useful microorganisms and enzymes.

[0037]The present process comprises the step of dissolving ascorbic acid
in glycerin at elevated temperature that deemed to be harmful and
degrading to ascorbic acid in the prior art.

[0038]It was pleasantly surprising to the inventor to discover that
vitamins dissolved in glycerin are stable even against elevated
temperatures that normally cause their degradation. Furthermore, it was
equally surprising to discover that heating ascorbic acid to temperatures
above 140 F when present in a glycerin solution does not cause loss of
strength or concentration of active vitamin C when performed at the
required water activity.

[0039]Conventionally, ascorbic acid is the most heat sensitive vitamin of
all vitamins. Moreover, liquid vitamin C solutions are extremely unstable
especially during extended storage. The inventor has discovered that
water activity has an important role in stabilizing vitamins particularly
at about 0.6 or under. Glycerin has been demonstrated to provide the best
protection at various water activities and temperatures.

[0040]To the ordinary skilled of the art it is well known that heating
vitamin C solution to elevated temperatures (about 130 F or above) will
damage the vitamin and should be avoided. No ordinary skilled in the art
will attempt to heat vitamin C solution to high temperature. Ascorbic
acid does not dissolve in glycerin at low temperature, however, the
inventor has discovered that heating ascorbic acid/glycerin solution
would cause minimal damage to ascorbic acid even when heated to about 165
F and above. Without any bearing on the findings or the applications, it
is speculated that because ascorbic acid is solubilized in glycerin which
provide humectancy, vitamin C is protected and in a state of inactivity.
In the presence of very low level of water, the degradation reaction is
slowed down significantly. Even though ascorbic acid is solubilized in
glycerin, it acts as if it is in a dry state. Dry ascorbic acid and
vitamin C powders are known to be more stable than liquid ones where the
vitamin is exposed to agents of degradation. Another speculative
explanation could be that the affinity of glycerin to form hydrogen bonds
with molecules of water will cause a reaction with the 2-hydroxy group
preventing ionization and thus preventing placing the two negative
charges in close proximity which favors ring stabilization and reduce
ring disruption. Furthermore, the proposed mechanism may reduce the
oxidative degeneration that usually occurs in the presence of water. It
is of particular importance to the inventor to discover that the above
mentioned stabilization mechanism is only achieved at elevated
temperatures. Glycerin does not support solubility of ascorbic acid at
ambient temperature. Heating is necessary to initiate and complete the
stabilization reaction.

[0041]The inventor has also discovered that other vitamins such as Vitamin
A (and its derivatives), Thiamin, Riboflavin, Niacin, Pantothenic Acid,
Cyanocobalamine, Folic Acid, Vitamin E, Vitamin D and Vitamin K are
protected against loss of activity and potency when various levels of
glycerin is present and in particular when the water activity is about
0.60 or below.

[0042]Furthermore, the inventor surprisingly discovered that the current
composition protects the vitality of natural color, fruit and vegetable
juices and flavor present. In addition, it was noticed that various
herbal preparations are preserved to a greater extent when added to the
current invention's formulation according the method and teaching of the
present invention. It appears that nutritional supplements are protected
by the presence of humectants low water activities. Since vitamin C is
the most sensitive vitamin, it is reasonable to assume that by protecting
vitamin C, other vitamins are protected similarly.

[0043]Suitable water for use in compositions in accordance with the
present disclosure include tap water and/or purified water such as for
example de-ionized water or USP water. As a non-limiting example, water
may be present in compositions in accordance with the present disclosure
in an amount of about 0% to about 50% by weight of the total composition.
In embodiments, water may be present in amounts of less than 10%, 20%,
30%, or 40% by weight of the total composition.

[0044]Suitable reducing sugars for use in compositions in accordance with
the present disclosure include sugars with a ketone or aldehyde group
such that the sugar is capable of acting as a reducing agent including
mannitol, sorbitol, xylitol, maltitol, lactitol, and/or combinations
thereof. In protecting vitamin C, it is believed that the reducing sugar
oxidizes first and delays the start of any oxidation of the vitamin C so
that excessive oxidation in water is delayed or totally avoided.
Optionally, the reducing sugars may be mixed with water to form a
reducing sugar solution that can be used to formulate a stable vitamin C
composition in accordance with this disclosure.

[0045]Propylene glycol is used as humectants and stabilizer (in prepared
fruits, vegetables and bakery goods) and as a solvent in flavor solutions
and extractions (and in food additives, such as colors, antioxidants,
enzymes and emulsifiers). It is also used as plasticizer and softening
agent for items such as cork seals. Propylene glycol has been used in
heat transfer fluids, beverage chilling and freezing applications,
solvents for printing inks used in food packaging and as equipment
cleaner, to remove contamination from food processing equipment In
countries of the European Union, propylene glycol is not cleared as a
general-purpose food grade product or direct food additive. The European
Council Directive 95/2/EC on food additives regulate its use in
foodstuffs for human consumption. Propylene glycol is cleared for use as
a carrier and carrier solvent in colors, emulsifiers, antioxidants and
enzymes at a maximum content of 1 gram per kilogram of final foodstuff.
Propylene glycol was assigned the E-number E1520.

[0046]In embodiments in accordance with the present disclosure, sorbitol,
maltitol, sodium lactate, corn syrup is used as humectant agents at 76%
of solution (W/W).

[0047]Glycerol is a chemical compound with the formula
HOCH2CH(OH)CH2OH. This colorless, odorless, viscous liquid is
widely used in pharmaceutical formulations. Also commonly called glycerin
or glycerin, it is a sugar alcohol, and is sweet-tasting and of low
toxicity. Glycerol has three hydrophilic alcoholic hydroxy groups that
are responsible for its solubility in water and its hygroscopic nature.
In foods and beverages, glycerol serves as humectant, solvent and
sweetener, and may help preserve foods. It is also used as filler in
commercially prepared low-fat foods (i.e., cookies), and as a thickening
agent in liquors. Glycerol also serves as a way, along with water, to
preserve certain types of leaves. Glycerol is also used as a sugar
substitute. In this regard, it has approximately 27 calories per teaspoon
and is 60% as sweet as sugar. Although it has about the same food energy
as table sugar, it does not raise blood sugar levels, nor does it feed
the bacteria that form plaques and cause dental cavities. As a food
additive, glycerol is also known as E422. Glycerol is used in medical and
pharmaceutical and personal care preparations, mainly as a means of
improving smoothness, providing lubrication and humectancy. It is found
in cough syrups, elixirs and expectorants, toothpaste, mouthwash, skin
care and soaps. It is also used as a substitute for ethanol as a solvent
in preparing herbal extractions. It is less extractive and is
approximately 30% less able to be absorbed by the body. Glycerin is used
at levels ranging from 36 to 86% to impact water activity levels ranging
from about 0.07 to 0.83.

[0048]Optionally, glycerin may be mixed with water to form a solution that
can be used to formulate a stable vitamin C composition in accordance
with this disclosure. The glycerin vitamin solution may contain, for
example, an amount of about 30% and about 95% by weight of the total
solution as glycerin. In other embodiments, reducing sugar solution may
contain about 76% by weight of the total reducing sugar solution.

[0049]The pH of the aqueous compositions in accordance with the present
disclosure may be adjusted to be about 1 to about 6, and, in some
particularly useful embodiments below 5. The pH of the composition
ensures that most of the ascorbic acid remains in the protonated,
uncharged form. The protonated form of ascorbic acid used in compositions
of the present disclosure is believed to remove the ionic repulsion of
the two oxygen groups, thus helping to stabilize the molecule. Agents
suitable for adjusting the pH of the aqueous phase include, but are not
limited to citric acid, phosphoric acid, lactic acid or glycolic acid.
The pH adjustment agents may be present in an amount of about 0.01% to
about 9% by weight of the total composition.

[0050]Suitable salt or derivative forms of vitamin C include any salt
formed from the neutralization of ascorbic acid. Non-limiting examples
include sodium ascorbate formed by the neutralization ascorbic acid with
sodium to form L-ascorbic acid-monosodium salt. Other non-limiting
examples of useful forms include calcium ascorbate, magnesium ascorbate,
potassium ascorbate, manganese ascorbate, zinc ascorbate, molybdenum
ascorbate, chromium ascorbate, and combinations thereof.

[0051]The vitamin C may be present in amounts that provide a benefit to
the health of a user. In embodiments, vitamin C is present in an amount
sufficient to promote therapeutic or corrective impact. The vitamin C
present may be in acidic form, salt form, or mixtures thereof. As an
illustrative example, vitamin C in amounts of about 5% to about 40% by
weight of the total composition may be suitable. In embodiments, vitamin
C is present in an amount of about 15% to about 25% by weight of the
total composition, and in some embodiments in amounts of about 1% to
about 22% by weight of the total composition.

[0052]The components of the composition are in a form that is systemically
ingestible in an animal or human. The components employed in the method
may be of various forms, consistencies or physical statuses. The
nutraceuticals compounds that could be utilized in the method may be
pre-hydrated, pre-solubilized, pre-coated, pre-encapsulated,
microencapsulated, micronized, particulate, micro-particulated or
prepared as timed-release components either individually or in various
combinations. The aqueous solution may further include water, one or more
reducing sugars, one or more herbs, one or more vitamins, one or more
surfactants, one or more flavors, one or more plant extracts such as
phytosterols, and combinations thereof.

[0053]The present composition and method can employ numerous types of
vitamins, probiotics, enzymes, hormones, nutritional supplements
synthetic compounds or other nutritional compounds and mixtures thereof
in various forms and shapes.

[0055]Optionally, the present liquids can include effective amounts of
flavor(s). If present, such flavors can comprise effective amounts of
flavors to provide desired flavor levels. Generally, flavors present at
from about 0.01% to about 10% of the finished products are contemplated.

[0056]Suitable non-nutritive sweeteners may also be used for sugar-free
fictional foods. Example of non-nutritive sweeteners includes Sucralose,
Aspartame, Saccharin and other high potency sweeteners. Suitable
materials for use as nutritive carbohydrate sweetening agents are well
known in the art. Examples of sweetening agents include both
monosaccharide and disaccharide sugars such as sucrose, invert sugar,
dextrose, lactose, honey, maltose, fructose, maple syrup and corn syrup
or corn syrup solids. Example nutritive carbohydrate sweetening agents
include those selected from the group consisting of sucrose, glucose,
fructose, and corn syrup solids. Suitable materials for use in the
current invention are those liquids and fluids with minimal amount of
water (about 30% or less). Example of other sweeteners is polyols (also
referred to as sugar alcohols, part of polyols' chemical structure
resembles sugar and part is similar to alcohols, the terms polyhydric
alcohols and polyalcohols may also be used). Polyols group includes
maltitol, sorbitol, xylitol, mannitol, isomalt and hydrogenated starch
hydrolysate. Other examples of suitable sweeteners are lactitol
monohydrate, and erythritol, syrups of sweeteners such as maltose,
fructose, glucose or natural syrups such as honey, maple syrup and corn
syrup.

[0057]The present compositions can optionally contain a variety of
additional ingredients suitable for rendering such products more
organoleptically acceptable, more nutritious and/or more storage stable.
Such optional components may include colors, coloring agents,
preservatives, emulsifiers, acidity and pH modifiers (acids and
alkaline). Of course, mixtures of the above-noted materials are
contemplated herein.

[0058]Any of processing vessels may be used to combine and heat-treat the
ingredients. A laboratory processor was utilized to impact mixing and
heating of components.

[0059]Any sequence of ingredients addition may be adopted before the
incorporation of nutraceuticals. In one embodiment, water and glycerin
are added first to the processor. Next ascorbic acid is added with
continuous agitation. Heating is commenced to about 130°
F.-190° F. Upon the complete solubilizatin of vitamin C, the
temperature of the system may be reduced to about 80-115° F.
before the addition of nutraceuticals in order to minimize the
detrimental impact of heat on active ingredients if needed for heat
sensitive components (such as hormones, bacteria and enzymes). Fat and
water soluble neutraceutical preparations, flavors, sweeteners, acidity
modifiers, colors or other optional ingredients are then added.

[0060]The resultant pasteurized product has a flowable consistency
suitable for further filling into suitable containers. Cooling of the
finished product is optional.

[0061]The liquid concentrated supplement may be filled using any of the
filling equipment known to those skilled in the art of packaging
technology. The nutritionally functional product may be dispensed into
plastic, glass, foil, synthetic materials, and paper or like containers
or packages.

[0062]The nutritionally functional product may be additionally dispensed
into hermetically sealed packages for extended shelf life. Dispensing the
compositions into hermetically sealed unit dose offers portability,
rigidity, and formability. It also provides protection against moisture,
gas and microbiological contamination extending the shelf life of unit
dose.

[0063]The stabilized fluid preparations may be handled and distributed
either at room temperature, refrigerated or frozen depending on the type
of nutraceutical compounds, distribution channels and the end-user.

EXAMPLES

[0064]This invention is further illustrated by the following examples,
which are to be regarded as illustrative only, and in no way limit the
scope of the invention. The following non-limiting examples and data
illustrate various aspects and features relating to the method(s) and
resulting products/compositions of this invention, including the
surprising and unexpected modification, control and/or improvement of the
water activity level through use/incorporation of the humectants of this
invention.

Example 1

[0065]The solubility of ascorbic acid in various solvents and humectants
was examined. Liquid nutritional supplements were produced according to
the teachings of the present invention. The liquid nutritional
supplements were formulated using various solvents individually as shown
below. All ingredients were mixed together in a laboratory processor to
make 1000 grams batches. Glycerin (GL), propylene glycol (PG), sorbitol
(SR), maltitol (ML), corn syrup 63/43 (CS) and sodium lactate (SL) were
added at percentage (w/w) of ingredients as follows:

[0067]It was observed that sorbitol, maltitol and sodium lactate required
the least temperature as well as the shortest time to completely dissolve
ascorbic acid followed by propylene glycol. Corn syrup required the
highest temperature as well as the longest time. Glycerin required high
temperature (160 F) and 25 minutes to completely dissolve. It should be
noticed that sugar alcohols may readily dissolve ascorbic acid at low
temperature with constant steering. In the case of glycerin, if
temperature is not raised, ascorbic acid will remain undissolved and
precipitate at the bottom of the beaker. That renders using glycerin
unobvious for the ordinary skilled in the art because heat damages
vitamin C severely as documented in the literature. Glycerin,
surprisingly produced the lowest water activity (Aw) of 0.296 after
dissolving ascorbic acid.

Example 2

[0068]Example 2 illustrates the stability of ascorbic acid of various
solvents containing dissolved vitamin C. About 12 grams of the liquid
nutritional supplements produced according to example 1, were dispensed
into hermetically sealed ampoules. The film used in thermoforming the
ampoules was manufactured using PCV/PE resin and contained no dyes to
provide a clear film with transparent properties to observe changes in
appearance. Three ampoules filled with various solutions containing
ascorbic acid were incubated at about 140 F for 11 days. Bubble formation
(sign of vitamin C decarboxylation) bloating of ampoules (sign of vitamin
C degradation) and color changes (sign of Vitamin C instability) were
recorded.

[0072]Only glycerin and propylene glycol showed stability during the 11
days incubation at high temperature with glycerin outperforming propylene
glycol after 5 days. It was surprising to discover that propylene glycol
may stabilize vitamin C longer than other humectants even though it did
not lower the water activity to a great extent. It is the inventor's
experience that one day at 140 F may correspond to one month of shelf
stability at ambient temperature. Based on the unexpected results, it
appears that glycerin is the optimal humectant to stabilize vitamins in
general and vitamin C in particular. Ampoules and other small packages
show signs of bloating and expand until bursting occur (seal failure).
Gas production is another observation of evident degradation of vitamin
C. In destabilized single doses, gas bubbles may be seen rising to the
top of the package leading to deformation of the package and eventually
bursting of package. The explosion and package seal failure will impact a
costly economic loss when nutritional supplements are shipped and stored
especially at hot climates. Increased stability of nutritional
supplements as taught in the current invention is of great economic
value. Additionally, glycerin is the solvent of choice because of less
desirable characteristics associated with propylene glycol. A mixture of
glycerin and other humectants and propylene glycol may be also of
advantage to stabilize vitamin C.

Example 3

[0073]To further evaluate the impact of various levels of glycerin on
water activity and dissolution parameters of vitamin C, the following
perpetrations were developed:

[0075]Water activity decreased as the amount of glycerin increased. The
higher the amount of glycerin, the higher the temperature of
incorporation required and the longer the time required. In order to
achieve a low level of water activity of about 0.80 or below, it was
concluded high levels of glycerin (about 46%) and temperature of above
the detrimental temperature (135 F) are required. To achieve complete
solubilization at that temperature, about 6 minutes of heat exposure is
needed which in a conventional solution may severely damage vitamin C. To
obtain lower water activity, a more detrimental treatment is needed which
may as documented in the literature irreversibly degrade vitamin C.

Example 4

[0076]Table 6, demonstrates the recovery of added vitamin C at various
water activities, temperature and minutes. Glycerin solutions prepared as
in example 3 were analyzed for vitamin C recovery.

[0077]All preparations exhibited remarkable recovery of vitamin C. By
incrementally lowering the water activity, no or little loss of vitamin C
occurred even as the temperature was raised to 165 F for an unusual
duration of 40 minutes. It was pleasantly surprising to discover that
vitamin C vitality could be preserved at high temperature for long time.
It is believed that this is the first time a heat sensitive nutrient
could be protected during processing.

Example 5

[0078]Example 5 illustrates the stability of ascorbic acid in various
concentrations of glycerin. About 12 grams of the liquid nutritional
supplements produced according to example 3, were dispensed into
hermetically sealed ampoules. The film used in thermoforming the ampoules
was manufactured using PCV/PE resin and contained no dyes to provide a
clear film with transparent properties to observe changes in appearance.
Three ampoules filled with various solutions containing ascorbic acid
were incubated at about 140 F for 30 days. Bubble formation (sign of
vitamin C decarboxylation) bloating of ampoules (sign of vitamin C
degradation) and color changes (sign of Vitamin C instability) were
recorded.

[0082]It could be concluded from the data above that the higher the
glycerin level (lower Aw) in the nutritional supplement, the more stable
vitamin C. Even glycerin levels of 45% may provide otherwise unattainable
shelf life equivalent to up to 5 month of active ascorbic acid. Even Aw
of 0.50 provided a long shelf life showing no further deterioration after
7 days (may be equivalent to 7 months on the retail shelves. Glycerin
concentration of 86% (w/w) and water activity of about 0.07 provided the
longest virtually unchanged appearance of vitamin C without apparent
color change or gas production. This surprising finding represents an
important stabilization technique to produce Vitamin C in hermetically
sealed packages. No bloating, gas production in a single serve sealed
package will occur, thus enabling to deliver concentrated forms of
vitamin C.

Example 6

[0083]Vitamin C was added to the glycerin formulation of example 3 at 5%
and 25% with the balance is compensated as water. Similar stability
results in sealed ampoules were obtained demonstrating that a wide range
of ascorbic acid concentrations may be utilized in the teaching of the
current invention without significant loss of activity.

Example 7

[0084]Utilizing a preparation of glycerin level of 60% and ascorbic acid
of 9%, various vitamins were added and analyzed for stability. Fat
soluble vitamins A and E were added at 2,500 IU and 30 IU respectively.
In a second group, water soluble vitamins Thiamine, Riboflavin, Niacin,
Pyridoxine, and Caynocolamine were added at 50% of daily values and
subjected to the heat treatment of about 160 F for 20 minutes. Water
activity was measured at 0.55 and pH at 2.0. Full recovery of added
vitamins was obtained emphasizing that if vitamin C is stabilized;
inherently other heat or water sensitive nutrients will be stabilized as
well.

Example 8

[0085]Utilizing a preparation of glycerin level of 40% and ascorbic acid
of 5%, various natural colors, juice concentrates and herbal extracts
were added and analyzed for stability. Echinacea and ginseng extracts,
pomegranate and carrot juice concentrates were added. Water activity was
measured at 0.80 and pH at 3.0. Upon incubation at 140 F for five days,
no color change of added juices had been noticed emphasizing that if
vitamin C is stabilized, inherently other heat or water sensitive
nutrients will be stabilized as well. Herbal extracts appeared to be not
affected by heat or incubation time.

Example 9

[0086]To a preparation of 70% glycerin and 20% ascorbic acid and 10%
water, about 0.3% of a blend of lipase and protease enzymes were added.
Water activity was measured at 0.13 and pH at 1.2. Incubation was
performed at 140 F for ten days. By adding the preparation to a base of
dairy ingredients and incubating the dairy base for 24 hrs, flavors and
tastes produced in the base were similar to the same dosage of enzyme
blend (0.3%) added directly to the base. It was concluded that the
process of the current invention may protect various enzymes against
deterioration.

Example 10

[0087]To the preparation of example 9, a blend of probiotics consisting of
L. acidophilus and L. burglarious was added to provide about one hundred
billion colonies per gram. Vitality was subjected to about 10 to 50% loss
during 7 days of incubation. It was concluded that the process of the
current invention may protect various microorganisms against death upon
extended storage conditions.

Example 11

[0088]The stability of ascorbic acid in a combination of various
humectants was examined. Liquid nutritional supplements were produced
according to the teachings of the present invention. The liquid
nutritional supplements were formulated using various humectants
combination as shown below. All ingredients were mixed together in a
laboratory processor to make 1000 grams batches. Glycerin (GL), propylene
glycol (PG), sorbitol (SR), maltitol (ML), and corn syrup 63/43 (CS) were
combined at percentage (w/w) of ingredients as follows:

[0089]Vitamin C dissolved satisfactorily in various combinations at about
165 F. Water activity ranged between 0.242 and 0.752. Combinations with
glycerin showed extended the shelf life more than the humectant alone.
Therefore, it could be concluded that glycerin is essential in lowering
the water activity when combined with other humectants or propylene
glycol.

[0090]While the principals of this invention have been described in
connection with specific embodiments, it should be understood clearly
that these descriptions, along with the chosen tables and data therein,
are made only by way of example and are not intended to limit the scope
of this invention, in any manner. Other advantages and features of this
invention will become apparent from the following claims, with the scope
thereof determined by the reasonable equivalents, as understood by those
skilled in the art.